反应详情

Imidazole (10.0 g, 146.9 mmol) was added to sodium hydride (60% dispersion in mineral oil, pre-washed in hexane, 6.5 g, 161.6 mmol) in DMF (200 ml), triphenylmethylchloride (41.0 g, 146.9 mmol) was then added and the reaction mixture stirred at room temperature for 18 h. The mixture was poured onto ice and the solid precipitate formed filtered off and partitioned between water and dichloromethane. The organic phase was washed with brine and dried over sodium sulphate and concentrated in vacuo to give the title compound (37.8 g, 83%). 1H NMR (CDCl3) δ 7.42-7.03 (1H, m). MS (ES) m/e 311 [M+H]+.

1. additionwas then added
2. additionThe mixture was poured onto ice
3. customthe solid precipitate formed
4. filtrationfiltered off
5. custompartitioned between water and dichloromethane
6. washThe organic phase was washed with brine
7. dry with materialdried over sodium sulphate
8. concentrationconcentrated in vacuo